Fast and quantitative determination of saxitoxin and neosaxitoxin in urine by ultra performance liquid chromatography-triple quadrupole mass spectrometry based on the cleanup of solid phase extraction with hydrophilic interaction mechanism
Abstract Saxitoxin (STX) and neosaxitoxin (NEO) are water-soluble toxins and their cleanup in bio-matrix is a hot topic but difficult problem. A fast and quantitative determination method for STX and NEO in urine was developed using ultra performance liquid chromatography-triple quadrupole mass spectrometry (LC–MS/MS) based on the cleanup of solid phase extraction (SPE) with hydrophilic interaction (HILIC) mechanism. Acetonitrile/methanol/water mixture was used to extract the toxins in urine. Polyamide (PA) was used as HILIC SPE material to clean the toxins in sample matrix. The limits of detection were 0.2ngmL −1 for STX and 1ngmL −1 for NEO in urine. The linear ranges were 0.5ngmL −1 –99.2ngmL −1 with the correlation coefficient of r = 0.9992 for STX and 2.1ngmL −1 –207ngmL −1 with r = 0.997 for NEO in urine matrix. The recoveries at three spiking levels were 81.5%–117% with the relative standard deviations (RSDs) of 5.4%–8.5% for STX and 89.0%–118% with the RSDs of 6.7%–9.1% for NEO. STX was found in all the 6 patients’ urines while NEO was only found in one sample from an intoxication case. Highlights STX and NEO in urine were analyzed by LC–MS/MS. The toxins were cleaned by HILIC SPE with polyamide material. HILIC SPE mechanism and the sample preparation procedure were discussed. STX and NEO were found in urine samples obtained from an intoxication case.
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